CN103426586A - Method for preparing zinc ferrite water-based nanometer magnetic fluid - Google Patents
Method for preparing zinc ferrite water-based nanometer magnetic fluid Download PDFInfo
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- CN103426586A CN103426586A CN2013103300906A CN201310330090A CN103426586A CN 103426586 A CN103426586 A CN 103426586A CN 2013103300906 A CN2013103300906 A CN 2013103300906A CN 201310330090 A CN201310330090 A CN 201310330090A CN 103426586 A CN103426586 A CN 103426586A
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Abstract
A method for preparing zinc ferrite water-based nanometer magnetic fluid includes the following steps of dispersing a certain weight of zinc ferrite nanometer particles into deionized water under the action of a dispersing agent, conducting stirring for a period of time under a constant first temperature to obtain dispersion fluid, and washing and adjusting the dispersion fluid to a certain pH value to obtain the zinc ferrite water-based nanometer magnetic fluid, wherein the first temperature ranges from 60 DEG C to 80 DEG C, the period of time ranges from 6 hours to 8 hours, and the certain pH value ranges from 8 to 11. The invention particularly relates to the method for preparing the zinc ferrite water-based nanometer magnetic fluid through the two steps. According to the method for preparing the zinc ferrite water-based nanometer magnetic fluid, a surface active agent is used for conducting surface modification on nanometer particles, therefore, nanometer fluid with better stability can be obtained, the zinc ferrite water-based nanometer magnetic fluid can not settle down after being placed in a base solution for one month, the granularity of the nanometer fluid obtained through preparation is very small, and a pipeline can not be easily blocked by the nanometer fluid.
Description
Technical field
The present invention is specifically related to a kind of employing two-step method, prepares the method for zinc ferrite water-base nano magnetic fluid.
Background technology
Convective heat transfer is in electric power, chemistry, air-conditioning, transportation and electron trade extensive application, and wherein heat-transfer working medium plays an important role.Heat-transfer working medium commonly used has water, mineral oil and ethylene glycol etc., and the conductive coefficient of these working medium is all lower, and heat transfer property is poor, becomes gradually one of major obstacle of convective heat transfer application.
Research shows that nano-fluid that applying nano materials is made into can significantly improve the heat transfer property of matrix, can be used as a kind of evenly, the Novel heat transfer working medium of stable, high thermal conductivity coefficient.Magnetic fluid is that absorption has magnetic particle highly dispersed in base load liquid of surfactant to distribute and the stable colloid system of formation.It not only has ferromagnetism, also has the mobility of liquid.It can stable for extended periods of time under the effect of gravity and electromagnetic force, not there will be precipitation or lamination.
Ferrite and composite nano materials thereof are the important multifunctional materials of a class, have very important researching value.Nanometer magnetofluid is compared with traditional heat transfer medium, not only has heat transfer property preferably, and have suspension stability good, do not stop up and the pipeline that weares and teares, etc. advantage.
Spinel zinc ferrite is nanocrystalline has the characteristics such as good magnetics, magneto-optic, catalysis, absorbing property and high chemical stability, with low cost, preparation technology is simple, and the size of magnetic can be along with the size of particle, the kind of metal and the difference of doping change and change, there is different character, and then be with a wide range of applications.Magnetic ferrous acid zinc nanoparticles has purposes widely, as contrast imaging, microwave absorbing material and the magnetic fluid etc. for magnetic recording material, magnetic immuno cell separation, nulcear magnetic resonance (NMR).Although the existing a large amount of report of the research of nano fluid heat transferring aspect, about the ferrite nano magnetic fluid in the research aspect heat transfer also in the starting stage.
The preparation method of nano-fluid mainly is divided into single-step method and two-step method.The especially applicable preparation of single-step method has the nano-fluid that is dispersed with metal nanoparticle of high thermal conductivity coefficient.The method of some gas phase synthesizing nano-particles, as vacuum vapor deposition, low-pressure gas evaporation, induced with laser chemical gaseous phase deposition method and energising heating vaporization etc., only need to change original gatherer, replace with the container that fills base fluid, just can directly prepare nano-fluid.The method program that two-step method prepares nano-fluid is simple, convenient, almost is applicable to the preparation of the nano-fluid of all kinds, and some height of usining that can make that single-step method is difficult to obtain shake the liquid of Kia as the nano-fluid of family estate.Along with the development of nanometer technology, can directly on market, buy the nano particle powder of different materials, make two-step method become more common nano-fluid preparation method.
Preparing on the method for nano-fluid, mostly adopt two-step method, but the zinc ferrite particle prepared at present is not little at present, stability is inadequate, long-time rear easily sedimentation in base fluid.
Summary of the invention
The invention provides a kind of method for preparing zinc ferrite water-base nano magnetic fluid, adopted surfactant, nano particle is carried out to surface modification, can obtain the good nano-fluid of stability, in base fluid, placing one month can sedimentation, and the nano-fluid particle prepared is very little, is difficult for blocking pipe.
In order to achieve the above object, the present invention has adopted following technical scheme:
A kind of method of utilizing the zinc ferrite nano particle to prepare zinc ferrite water-base nano magnetic fluid, there is such feature, comprise following steps: get during certain mass zinc ferrite nano particle is distributed to deionized water under the dispersant effect, at the first temperature, constant temperature stirs a period of time, obtains dispersion liquid; Dispersion liquid is washed and is adjusted to certain pH value, obtain zinc ferrite water-base nano magnetic fluid, the scope of the first temperature is 60 ℃-80 ℃, and a period of time is 6-8 hour, and the scope of certain pH value is 8-11.
Further, the method for preparing zinc ferrite water-base nano magnetic fluid of the present invention can also have such feature: dispersant is any one or the combination in PEG-4000, polyacrylic acid, polyacrylate, oleate.
Further, the method for preparing zinc ferrite water-base nano magnetic fluid of the present invention can also have such feature: the 2-3 that the quality of dispersant is the zinc ferrite nano particle doubly.
Further, the method for preparing zinc ferrite water-base nano magnetic fluid of the present invention can also have such feature: the scope of certain pH is 10-11.
Further, the method for preparing zinc ferrite water-base nano magnetic fluid of the present invention can also have such feature: the mass fraction of zinc ferrite water-base nano magnetic fluid is 0.1-0.5%.
Further, the method for preparing zinc ferrite water-base nano magnetic fluid of the present invention, can also have such feature, the preparation method of zinc ferrite nano particle comprises the following steps: white vitriol and ferrous sulfate heptahydrate are dissolved in deionized water with certain mol proportion, obtain the first solution; Add hexa-methylene Four Modernizations amine in the first solution, be adjusted to certain pH value, obtain the second solution; By the second solution heated at constant temperature certain hour at the first temperature, obtain the 3rd solution; By the 3rd solution carry out cooling after, washed and collected reactant, obtain the zinc ferrite nano particle; Wherein, mol ratio is 1:2, and the scope of the first temperature is 120 ℃-180 ℃, and certain hour is 6-20 hour.
Further, the method for preparing zinc ferrite water-base nano magnetic fluid of the present invention can also have such feature: in the first solution, the molar concentration of white vitriol is 0.005-0.02m/L.
Further, the method for preparing zinc ferrite water-base nano magnetic fluid of the present invention can also have such feature: also need to add any one or combination in natrium citricum, NaOH and urea in the first solution.
In addition, the method for preparing zinc ferrite water-base nano magnetic fluid of the present invention can also have such feature: the first temperature range is 160 ℃.
Effect and the effect of invention
According to the method for preparing zinc ferrite water-base nano magnetic fluid the present invention relates to, adopted surfactant, nano particle is carried out to surface modification, can obtain the good nano-fluid of stability, in base fluid, placing one month can sedimentation, and the nano-fluid particle prepared is very little, is difficult for blocking pipe; Simultaneously raw material is simple, just can obtain corresponding ferrite not introducing external oxidant, and preparation process is simple, and the operation facility, reduced preparation cost; Temperature required low-temperature hydrothermal-solvent heat the category that belongs to, low for equipment requirements; Applied widely, the kind of the temperature of reacting by change and reaction time, additive and the kind of alkali can be regulated and controled the pattern granular size of product, prepare nanoscale and micron-sized crystal grain.The zinc ferrite water-base nano magnetic fluid that the present invention prepares is the superparamagnetic material, and self magnetic is weak but magnetic response is high.
The accompanying drawing explanation
The TEM shape appearance figure that Fig. 1 is the zinc ferrite water-base nano magnetic fluid that obtains in embodiment mono-;
The TEM shape appearance figure that Fig. 2 is the zinc ferrite water-base nano magnetic fluid that obtains in embodiment bis-;
The TEM shape appearance figure that Fig. 3 is the zinc ferrite water-base nano magnetic fluid that obtains in embodiment tri-;
The TEM shape appearance figure that Fig. 4 is the zinc ferrite water-base nano magnetic fluid that obtains in embodiment tetra-;
The TEM shape appearance figure that Fig. 5 is the zinc ferrite water-base nano magnetic fluid that obtains in embodiment five;
The XRD collection of illustrative plates that Fig. 6 is the zinc ferrite water-base nano magnetic fluid that obtains under the differential responses time in embodiment six;
Fig. 7 adds in embodiment six and the Fourier infrared spectrum figure of the zinc ferrite water-base nano magnetic fluid that do not obtain under same reaction conditions while not adding dispersant; And
The B-H loop that Fig. 8 is the zinc ferrite water-base nano magnetic fluid that obtains under the differential responses time in six in embodiment.
Embodiment
Embodiment mono-
1mmol white vitriol and 0.5mml ferrous sulfate heptahydrate are dissolved in the 70mL deionized water, add again hexa-methylene Four Modernizations amine and NaOH, regulating the pH value is 8, the solution obtained is contained in the closed container of heat-resistant pressure-resistant, 120 ℃ of heated at constant temperature 8 hours, after closed container is cooled to room temperature, takes out solution and also washed three times in thermostatic drying chamber, collect reactant, obtain the zinc ferrite nano particle.
Get 0.1g ZnFe
2O
4The zinc ferrite nano particle is put into there-necked flask, add water 300mL, warming-in-water is to 60 degree, add 1g enuatrol and 1g PEG-4000 mixed solution 100mL, mechanical agitation 6 hours, washed the dispersion liquid after stirring three times, then the pH value be adjusted to 8, and add deionized water to 100mL, obtain zinc ferrite water-base nano magnetic fluid.
Outwell supernatant after can inhaling lower precipitated product with magnet during washing, carry out again ultrasonic dispersion to wash next time after also can adopting centrifugation.
The TEM shape appearance figure that Fig. 1 is the zinc ferrite water-base nano magnetic fluid that obtains in embodiment 1.
In the present embodiment, the TEM shape appearance figure of resulting zinc ferrite water-base nano magnetic fluid product as shown in Figure 1, is particle shape nano material.
The XRD collection of illustrative plates that Fig. 6 is the zinc ferrite water-base nano magnetic fluid that obtains under the differential responses time in embodiment, wherein, the XRD collection of illustrative plates that the b curve is the zinc ferrite water-base nano magnetic fluid that obtains in embodiment 1.
In the present embodiment, the X ray diffracting spectrum of resulting zinc ferrite water-base nano magnetic fluid product is as shown in b curve in Fig. 6, can find out at this temperature, X ray diffracting spectrum part peak position is consistent with the ZnFe2O4 in international standard spectrogram storehouse, by calculating, the average-size of nano particle is 20～30nm.
Embodiment bis-
1mmol white vitriol and 0.5mml ferrous sulfate heptahydrate are dissolved in the 70mL deionized water, add again hexa-methylene Four Modernizations amine and natrium citricum, regulating the pH value is 9, the solution obtained is contained in the closed container of heat-resistant pressure-resistant, 140 ℃ of heated at constant temperature 12 hours, after closed container is cooled to room temperature, takes out solution and also washed three times in thermostatic drying chamber, collect reactant, obtain the zinc ferrite nano particle.
Get 7g ZnFe
2O
4The zinc ferrite nano particle is put into there-necked flask, add water 300mL, warming-in-water is to 70 degree, add 7g enuatrol and 7g PEG-4000 mixed solution 100mL, mechanical agitation 7 hours, washed the dispersion liquid after stirring three times, then the pH value be adjusted to 9, and add deionized water to 2L, obtain zinc ferrite water-base nano magnetic fluid.
Outwell supernatant after can inhaling lower precipitated product with magnet during washing, carry out again ultrasonic dispersion to wash next time after also can adopting centrifugation.
The TEM shape appearance figure that Fig. 2 is the zinc ferrite water-base nano magnetic fluid that obtains in embodiment 2.
In the present embodiment, the TEM shape appearance figure of resulting zinc ferrite water-base nano magnetic fluid product as shown in Figure 2, is particle shape nano material.
The XRD collection of illustrative plates that Fig. 6 is the zinc ferrite water-base nano magnetic fluid that obtains under the differential responses time in embodiment, wherein, the XRD collection of illustrative plates that the c curve is the zinc ferrite water-base nano magnetic fluid that obtains in embodiment 2.
In the present embodiment, the X ray diffracting spectrum of resulting zinc ferrite water-base nano magnetic fluid product is as shown in c curve in Fig. 6, can find out at this temperature, X ray diffracting spectrum part peak position is consistent with the ZnFe2O4 in international standard spectrogram storehouse, by calculating, the average-size of nano particle is 30～40nm.
Embodiment tri-
10mmol white vitriol and 5mml ferrous sulfate heptahydrate are dissolved in the 350mL deionized water, add again hexa-methylene Four Modernizations amine and natrium citricum, regulating the pH value is 10.5, the solution obtained is contained in the closed container of heat-resistant pressure-resistant, 160 ℃ of heated at constant temperature 18 hours, after closed container is cooled to room temperature, takes out solution and also washed three times in thermostatic drying chamber, collect reactant, obtain the zinc ferrite nano particle.
Get 7g ZnFe
2O
4The zinc ferrite nano particle is put into there-necked flask, add water 300mL, warming-in-water is to 70 degree, add 7g enuatrol and 7g PEG-4000 mixed solution 100mL, mechanical agitation 8 hours, washed the dispersion liquid after stirring three times, then the pH value be adjusted to 10.5, and add deionized water to 2L, obtain zinc ferrite water-base nano magnetic fluid solution.
Outwell supernatant after can inhaling lower precipitated product with magnet during washing, carry out again ultrasonic dispersion to wash next time after also can adopting centrifugation.
The TEM shape appearance figure that Fig. 3 is the zinc ferrite water-base nano magnetic fluid that obtains in embodiment 3.
In the present embodiment, the TEM shape appearance figure of resulting zinc ferrite water-base nano magnetic fluid product as shown in Figure 3, is particle shape nano material.
The XRD collection of illustrative plates that Fig. 6 is the zinc ferrite water-base nano magnetic fluid that obtains under the differential responses time while in embodiment, adding natrium citricum, wherein, the XRD collection of illustrative plates that the d curve is the zinc ferrite water-base nano magnetic fluid that obtains in embodiment 2.
In the present embodiment, the X ray diffracting spectrum of resulting zinc ferrite water-base nano magnetic fluid product is as shown in d curve in Fig. 6, can find out at this temperature, X ray diffracting spectrum part peak position is consistent with the ZnFe2O4 in international standard spectrogram storehouse, by calculating, the average-size of nano particle is 35～50nm.
Embodiment tetra-
10mmol white vitriol and 5mml ferrous sulfate heptahydrate are dissolved in the 350mL deionized water, add again hexa-methylene Four Modernizations amine and natrium citricum, regulating the pH value is 11, the solution obtained is contained in the closed container of heat-resistant pressure-resistant, 180 ℃ of heated at constant temperature 20 hours, after closed container is cooled to room temperature, takes out solution and also washed three times in thermostatic drying chamber, collect reactant, obtain the zinc ferrite nano particle.
Get 7g ZnFe
2O
4The zinc ferrite nano particle is put into there-necked flask, add water 300mL, warming-in-water is to 70 degree, add 7g aqueous solution sodium oleate 50mL, add afterwards 7g polyacrylic acid sodium water solution 50mL, mechanical agitation 8 hours, dispersion liquid after stirring is washed three times, again the pH value is adjusted to 11, and adds deionized water to 2L, obtain zinc ferrite water-base nano magnetic fluid solution.
Outwell supernatant after can inhaling lower precipitated product with magnet during washing, carry out again ultrasonic dispersion to wash next time after also can adopting centrifugation.
The TEM shape appearance figure that Fig. 4 is the zinc ferrite water-base nano magnetic fluid that obtains in embodiment 4.
In the present embodiment, the TEM shape appearance figure of resulting zinc ferrite water-base nano magnetic fluid product as shown in Figure 4, is particle shape nano material.The particle extent of polymerization increases to some extent than embodiment 1～3, and the particle diameter calculated is compared with embodiment 1～3 also to be increased to some extent, is 50～70nm.
Embodiment five
10mmol white vitriol and 5mml ferrous sulfate heptahydrate are dissolved in the 350mL deionized water, add again hexa-methylene Four Modernizations amine and natrium citricum, regulating the pH value is 11, the solution obtained is contained in the closed container of heat-resistant pressure-resistant, 160 ℃ of heated at constant temperature 12 hours, after closed container is cooled to room temperature, takes out solution and also washed three times in thermostatic drying chamber, collect reactant, obtain the zinc ferrite nano particle.
Get 7g ZnFe
2O
4The zinc ferrite nano particle is put into there-necked flask, add water 300mL, warming-in-water, to 80 degree, is added 7g aqueous solution sodium oleate 50mL, adds afterwards 7g PEG aqueous solution 50mL, mechanical agitation, 8 hours, the dispersion liquid after stirring is washed three times, then the pH value is adjusted to 11, and add deionized water to 2L, obtain zinc ferrite water-base nano magnetic fluid solution.
Outwell supernatant after can inhaling lower precipitated product with magnet during washing, carry out again ultrasonic dispersion to wash next time after also can adopting centrifugation.
The TEM shape appearance figure that Fig. 5 is the zinc ferrite water-base nano magnetic fluid that obtains in embodiment 5.
In the present embodiment, the TEM shape appearance figure of resulting zinc ferrite water-base nano magnetic fluid product as shown in Figure 5, is particle shape nano material.The particle extent of polymerization increases to some extent than embodiment 1～3, and the particle diameter calculated is compared with embodiment 1～3 also to be increased to some extent, is 45～70nm.
Embodiment six
1mmol white vitriol and 0.5mml ferrous sulfate heptahydrate are dissolved in the 70mL deionized water, add again hexa-methylene Four Modernizations amine and natrium citricum, regulating the pH value is 9, the solution obtained is contained in the closed container of heat-resistant pressure-resistant, 160 ℃ of heated at constant temperature 6,12,16 hours respectively, after closed container is cooled to room temperature, takes out solution and also washed three times in thermostatic drying chamber, collect reactant, obtain the zinc ferrite nano particle.
Get 7g ZnFe
2O
4The zinc ferrite nano particle is put into there-necked flask, add water 300mL, warming-in-water is to 70 degree, add 7g enuatrol and 7g PEG-4000 mixed solution 100mL, mechanical agitation 7 hours, washed the dispersion liquid after stirring three times, then the pH value be adjusted to 9, and add deionized water to 2L, obtain zinc ferrite water-base nano magnetic fluid.
Outwell supernatant after can inhaling lower precipitated product with magnet during washing, carry out again ultrasonic dispersion to wash next time after also can adopting centrifugation.
Fig. 7 adds in embodiment six and the Fourier infrared spectrum figure of the zinc ferrite water-base nano magnetic fluid that do not obtain under same reaction conditions while not adding dispersant, wherein, Fourier's infrared spectrogram that a curve is the 0.5mmol sample that obtains in situation in 16 hours of 160 degree; The b curve is 160 degree is coated with the 0.5mmol sample of sour sodium and PEG-4000 acquisition in 16 hours Fourier's infrared spectrogram in situation.
The Fourier infrared spectrum figure contrast that coats upper organic group while adding PEG-4000 and enuatrol as dispersant in embodiment six and do not coat the resulting zinc ferrite water-base nano of organic group magnetic fluid as shown in Figure 7, do dispersant with PEG-4000 and enuatrol and can allow zinc ferrite water-base nano magnetic fluid sample coat the last layer organic substance, increased the suspension that nano particle makes fluid.
The B-H loop that Fig. 8 is the zinc ferrite water-base nano magnetic fluid that obtains under the differential responses time in embodiment six, the B-H loop that wherein a curve is the 0.5mmol sample that obtains in situation in 6 hours of 160 degree; The B-H loop that the b curve is the 0.5mmol sample that obtains in situation in 12 hours of 160 degree.
The B-H loop of the zinc ferrite water-base nano magnetic fluid obtained under the differential responses time as shown in Figure 8, illustrate that the nanometer magnetofluid made is superparamagnetic material.
The effect of embodiment and effect
The method for preparing zinc ferrite water-base nano magnetic fluid related to according to the present embodiment, it has adopted surfactant, nano particle is carried out to surface modification, can obtain the good nano-fluid of stability, in base fluid, placing one month can sedimentation, and the nano-fluid particle prepared is very little, is 20～70nm, is difficult for blocking pipe.
Simultaneously, the raw material that preparation method in embodiment adopts is simple, just can obtain corresponding ferrite not introducing external oxidant, and preparation process is simple, and the operation facility, reduced preparation cost; Temperature required low-temperature hydrothermal-solvent heat the category that belongs to, low for equipment requirements.
In addition, the preparation method's in the present embodiment is applied widely, and the kind of the temperature of reacting by change and reaction time, additive and the kind of alkali can be regulated and controled the pattern granular size of product, prepare nanoscale and micron-sized crystal grain.The zinc ferrite water-base nano magnetic fluid that the present invention prepares is the superparamagnetic material, and self magnetic is weak but magnetic response is high.
Claims (9)
1. a method of utilizing the zinc ferrite nano particle to prepare zinc ferrite water-base nano magnetic fluid, is characterized in that, comprises following steps:
Get during the described zinc ferrite nano particle of certain mass is distributed to deionized water under the dispersant effect, at the first temperature, constant temperature stirs a period of time, obtains dispersion liquid;
Described dispersion liquid is washed and is adjusted to certain pH value, obtained described zinc ferrite water-base nano magnetic fluid,
Wherein, the scope of described the first temperature is 60 ℃-80 ℃,
Described a period of time is 6-8 hour,
The scope of described certain pH value is 8-11.
2. the method for preparing zinc ferrite water-base nano magnetic fluid according to claim 1 is characterized in that:
Wherein, described dispersant is any one or the combination in PEG-4000, polyacrylic acid, polyacrylate, oleate.
3. the method for preparing zinc ferrite water-base nano magnetic fluid according to claim 1 is characterized in that:
Wherein, the 2-3 that the quality of described dispersant is described zinc ferrite nano particle doubly.
4. the method for preparing zinc ferrite water-base nano magnetic fluid according to claim 1 is characterized in that:
Wherein, the scope of described certain pH is 10-11.
5. the method for preparing zinc ferrite water-base nano magnetic fluid according to claim 1 is characterized in that:
Wherein, the mass fraction of described zinc ferrite water-base nano magnetic fluid is 0.1-0.5%.
6. the method for preparing zinc ferrite water-base nano magnetic fluid according to claim 1, is characterized in that, the preparation method of described zinc ferrite nano particle comprises the following steps:
White vitriol and ferrous sulfate heptahydrate are dissolved in deionized water with certain mol proportion, obtain the first solution;
Add hexa-methylene Four Modernizations amine in described the first solution, be adjusted to described certain pH value, obtain the second solution;
By described the second solution heated at constant temperature certain hour at the first temperature, obtain the 3rd solution;
By described the 3rd solution carry out cooling after, washed and collected reactant, obtain described zinc ferrite nano particle;
Wherein, described mol ratio is 1:2,
The scope of described the first temperature is 120 ℃-180 ℃,
Described certain hour is 6-20 hour.
7. the method for preparing zinc ferrite water-base nano magnetic fluid according to claim 6 is characterized in that:
Wherein, described in described the first solution, the molar concentration of white vitriol is 0.005-0.02m/L.
8. the method for preparing zinc ferrite water-base nano magnetic fluid according to claim 6 is characterized in that:
Wherein, also need to add any one or the combination in natrium citricum, NaOH and urea in described the first solution.
9. the method for preparing zinc ferrite water-base nano magnetic fluid according to claim 6 is characterized in that:
Wherein, described the first temperature range is 160 ℃.
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| CN111977696B (en) * | 2020-08-13 | 2022-06-07 | 吉林化工学院 | Preparation method and application of pomegranate-shaped magnetic visible light heterogeneous Fenton catalyst material |
| CN112028127A (en) * | 2020-09-17 | 2020-12-04 | 甘肃农业大学 | Rheological phase synthesis method of nano zinc ferrite |
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